Hydroxyamine hydrochloride → HCID 73509154, compound

Participants

Reaction Steps

To a solution of the title compound of Example H (3.16 g, 10.8 mmol) in pyridine (50 ml) was added hydroxylamine hydrochloride (3.73 g, 54. mmol) and the reaction was stirred for 5 days(d) at room temperature. After the reaction was concentrated in vacuo, HO was added and the mixture was extracted with CH2Cl2. Drying of the organic phase (MgSO4) and concentration gave a solid which was chromatographed on silica gel eluting with 2% EtOH/CH2Cl2 to give the title compound (1.91 g, 57%). Anal calcd for C15H17N2O4F: C, 58.44; H, 5.56; N, 9.09. Found: C, 58.43; H, 5.62; N, 8.75. DSC=175.1°-180.2° C. at 225.6 J/g.

Provenance & Evidence